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Be methodical. And take notes. Working helter-skelter gets helter-skelter results. And
often a miss instead of a hit. And if you don’t take notes you may not remember
exactly what you did to get the results you got – good or bad. It’s nice to be able to
repeat the good tests – avoid the bad ones. Notes help guide you in that direction.
Keep them to refer back to the next time you test something. It might be a year
between doing certain tests for certain things – and those notes will be worth their
weight in gold as reminders.
There are basically two broad categories into which tests fall: Qualitative and
quantitative. Qualitative tests tell you whether or not a certain element, radical, or
compound is present in your mystery mineral. Quantitative tests tell you how much of
that constituent is present – weight percents or mole percents of various elements or
oxides of elements, etc. Quantitative tests are rather tricky – or at least reliable ones
are. They are “advanced mineral chemistry.” We’ll stick to qualitative tests for this
basic introduction to home lab work, with maybe some hints on rough quantitative
measurements now and then. You’re interested in seeing what the mystery mineral
contains, not how much of it or how pure the sample is. At least that should be the
focus when you start out. Any quantitative hints that get discussed will serve to point
out that there is that next level of chemistry available – when you feel up to moving
on.
In qualitative testing the goal is to find out whether or not certain constituents are in
the mystery mineral. If you suspect a calcium-bearing mineral, you test to see if there
really is calcium present. And so on. Most of the tests we’ll discuss here are of that
type. Is it – or isn’t it – present? Negative results are as important as positive ones.
They tell you what isn’t present. So you can move on to find out what is.
METHODOLOGY & THOROUGHNESS
You don’t need a home lab to identify minerals that can be identified from gross
physical features – such as quartz, kyanite, and muscovite (usually…) Save the lab
work for stuff that is defying identification by simpler means. Except it’s not a bad
idea to experiment on “knowns” – see if you can “prove” a pyrite sample is pyrite by
chemical testing. Same with other species you are familiar with. The practice will
familiarize you with testing procedures, give you experience working with the
chemicals, and give you some confidence once you get things worked out and are
“proving” the samples are what you know they are. But, by-and-large, save the lab
work for the tough ones.
As stated in the previous post, lab tests are all about finding out what’s in your
mystery mineral(s). You narrow down the possibilities to two or a few species, and
then you say “Okay – now what are the chemical differences between these species
that I can test for to figure out which I have?” Let’s take a simple example: You have
a sample that you’ve narrowed down to being one of the following species: calcite,
magnesite, siderite, or smithsonite. Normally, figuring out the specific gravity of the
mineral would tell you which you have – but your sample is small crystals, nothing
big enough for you to work with on the triple beam balance (or whatever you use to
do S.G. tests.) So you look these species up and find that calcite is CaCO3, magnesite
is MgCO3, siderite is FeCO3, and smithsonite is ZnCO3. The only difference between
these species is their metallic ion: Ca, Mg, Fe and Zn. So the way to find out which
species you have is to test for those ions – find out which is present. You therefore
need a chemical test that will identify Ca, another that will identify Mg, and so on…
A simple chemical test for Ca is to dissolve a pinch of the powdered sample in a drop
or two of hydrochloric acid (HCl) and then add sodium sulfate (Na2SO4) to the
solution. If you get a white precipitate (it’s CaSO4) there is Ca in the sample. It’s
probably calcite. BUT – a single test is not conclusive. Any of these minerals may
have Ca in them in small amounts as a “substitution” for the principal metallic ion.
(We get the “ideal formulas” fed to us in books – not “actual formulas.”) So you
would still need to test further. You can test for Mg by dissolving a pinch of the
powdered mineral in HCl and adding several drops of a strong solution of ammonia to
it. Then add a bit of Na2HPO4.12H2O to the solution. If you get a white precipitate
(it’s NH4MgPO4) then there is Mg in the sample. To test for Fe you could use any of
several test. One simple one is to dissolve a pinch of the powdered sample in a drop or
two of HCl and then add several drops of ammonia hydroxide (NH4OH) solution to it
to make it alkaline. If you get a tannish to white precipitate (it’s Fe(OH)3 ) then there
is Fe in the sample. Then, for Zn, dissolve a pinch of powdered sample in HCl and
add sodium disulfide (Na2S) solution – if you get a white precipitate (it’s ZnS) there’s
Zn in the sample.
As you do each test, observe the volume of precipitate formed – keep adding the
reagent to the solution (in tiny amounts) until no more reaction is taking place, no
more precipitate forming. (If you keep the slides (or test tubes) of each solution lined
up on the table, when all the tests are done you can compare the solutions with one
another directly if necessary.) Note any negative results – such as no Mg found. Those
eliminate species from your list of “likely suspects.” Let’s say you got negatives for
Ca and Mg, positives for Fe and Zn. But the Zn test barely showed a trace, while the
Fe test showed the sample is loaded with Fe. You’re “mystery mineral” is no longer a
mystery – it’s siderite with a little bit of Zn substituting for the Fe. Actual formula:
(Fe,Zn)CO3. “Ideal” formula: FeCO3. [And here we’ve looked at rough quantitative
testing: “How much?” As opposed to “Is it there?”]
“Aha!” Someone says. “But how do you know it is an iron *carbonate*? – not a
sulfate or something else?” Well – I said you’d already decided it had to be on of the
carbonates named. And you probably did that be testing a sample or two with HCl to
see if it “fizzed.” And it did… Which is another chemical test – a simple test for CO2
(which is what comes bubbling out of a solution of carbonate mineral and acid.) See –
you already knew one “chemical test” and didn’t even realize it! If you didn’t do that
test, and decided it must be one of those carbonates by other means, then that test
needs to be done to prove your guess is correct. Because without knowing for sure
that the mineral is a carbonate, it may well be something else, like a sulfate. (Actually,
if you think about it, you “proved” the mineral to be a carbonate as you dissolved the
powder in acid – because it bubbled as it dissolved… PS: The sulfates of Fe, Mg and
Zn are readily soluble in acids and likely to stay dissolved – not precipitate out of
solution. Another reason you’d know the mineral was a carbonate – not a sulfate - in
the above scenario.)
You have to test for EACH of the suspected constituents in a mineral – not just one.
Which can be tricky if you only have a little bit of powdered mineral to work with and
need to do a bunch of tests. Here the minimalist approach I recommend becomes
critical – else you may not be able to do all the tests needed. It is always a good idea
to figure out how many tests you are going to need to do and then divide up the
available mineral powder solution into that many “batches.” In some cases this may
mean that all you have to work with are a drop or two of solution for each test. A
micro-eyedropper is handy for working with tiny amounts of solutions – and you’ll
probably need to work under the microscope in order to see the reactions in the tiny
drops of solutions you have. But it can be done. You can also divide up the mineral
powder into tiny “piles” ahead of time and then make the solutions you need from
them. This is handy if you need different powder solutions for different tests. But it
can be tough to do with tiny quantities of powder – possibly ending up with just a few
grains of powder to make solutions from.
Of course not all tests are as simple as the series described above. Or all results as
certain as our hypothetical case. I picked an “easy” one to illustrate the methodology.
And to point out that you can’t just test for one thing and – if its positive – say
“Voila!” You can’t. You have to take other possibilities besides your “prime suspect”
into consideration. In the above case, if you’d just tested for Zn you would have
falsely concluded the mineral was smithsonite… Chemical testing is about “proving
your case beyond a reasonable doubt.” Any single test is more than likely to leave
plenty of room for doubt. Conclusive results come from being thorough – testing for
all possible culprits and finding out which you have, and which is the most likely
“prime candidate” based on comparisons.
MAKING SOLUTIONS
Nearly all of the tests require that you first dissolve some of the powdered mystery
mineral to make a solution that is then used for testing. This can be a problem in itself:
What do you use to dissolve the powder? (And here we are talking about *dissolving*
the powder – not just mixing it in liquid. In a mixture, the powder is not dissolved,
just stirred in and floating around. In a solution the powder has been dissolved –
broken up into its constituent ions.)
Only a few minerals are soluble in water – mostly halides and iodides. (Which can be
a quick test to see if you have one of those species.) But the odds are that your powder
won’t dissolve in water – you’ll have to try something else. Try hydrochloric acid
(HCl) first. A great many minerals will dissolve in HCl. If that doesn’t work, try nitric
acid (HNO3). If that doesn’t work, try sulfuric acid (H2SO4) last. If that doesn’t work
the odds are your mystery mineral is a silicate, few of which will dissolve in acids.
Zeolites do, and a few others, but by-and-large silicates are insoluble in anything short
of hydrofluoric acid (HF) – and that’s one acid you can’t play with at home. (It’s
extremely dangerous and requires special lab equipment – including a negative
pressure ventilation hood – to work with safely.) If you run through the list of acids
you can use at home and still can’t get the powder to dissolve, you’ve pretty much
determined the mineral is a silicate – and probably not a Zeolite. Important
information in itself.
A few other acids are also used in making solutions, such as acetic and oxalic. But
these are rather weak acids, comparatively speaking (they can still be “strong,” for
them, and are dangerous.) They are usually not used unless a specific test calls for
them. And if a test does call for one and you can’t get the powdered mineral to
dissolve in it, the odds are the mineral is not what you think it is and are testing for:
You can scratch that possibility and move on to other tests.
ACIDITY vs ALKALINITY
Quite a few of the tests require you to start with an acid solution and then make it
alkaline by adding a base, such as ammonium hydroxide (NH4OH). In some cases
you simply overload the solution with the base to get it there. In others you need to
work carefully to make the solution just slightly alkaline.
You use litmus paper for checking the pH of solutions. But since you are working
with such small quantities of liquids, you don’t want to just stick the tip of the test
strip in the solution – it might wick up your entire batch of liquid! Instead, dip a small
diameter (approx. 2.5 mm) glass rod in the solution and then touch the wetted end of it
to a fresh spot on the litmus paper. The wetted spot on the paper will then tell you
where things stand alkalinity wise.
Also, sometimes (though rarely) you need a neutral solution – pH of 7. Which can be
tricky to achieve. You pretty much need to use a micro-eyedropper to slowly add the
base and – drop by drop – neutralize the acid, testing your solution with a glass rod
and litmus paper after each drop has been added and stopping the first time the litmus
paper doesn’t turn color.
MAKING A MICRO-EYEDROPPER
You can buy eyedroppers with small diameter ends if you have a good chemical
supply house in your area. But otherwise they can be hard to come by – and they
aren’t really “micro” eyedroppers. So you might want to try and make your own. Take
an 8 inch length of glass tubing about the same diameter as a typical medicine
eyedropper. Heat the center of it over a propane torch flame until it’s soft. Then
remove it from the flame and pull on both ends so the middle stretches out. Snap the
middle – so there is a roughly 3 inch long thin capillary tube coming off the end of the
unstretched part of the tube. Once the glass has cooled, then heat the wide end of the
tube until it’s soft and flare it slightly with the tang of a file – so it looks roughly like
the top end of a regular medicine dropper. After it cools again, fit the flared end with a
medicine dropper bulb.
If done right, you get an eyedropper that has a very thin capillary tube on its end – just
right for creating micro-drops of solutions. Actually, one length of tubing can give
you two droppers if you do the stretching and snapping carefully – each half having a
capillary tube on its end. If you make several of them you’ll have enough to do testing
without having to clean one between use in different solutions. Just make sure they –
and all your glassware, etc. – get cleaned thoroughly between sessions. There’s
nothing like evaporated residue to botch up a test…
HEATING THINGS
First off, where a test calls for heating liquids on a glass microscope slide you need to
be very careful. If you just stick the slide over the flame the odds are it will shatter.
And you can’t just try to hold it immediately above the flame – because that happens
to be a pretty hot spot in the gas stream. You need to hold the slide “high” – two or
more inches above the flame. There’s enough heat at that point to slowly warm the
slide, but not so much that it will heat the slide quickly and shatter it. I suggest you
practice (with a broken half of a slide if you have a couple that you’ve dropped) and
use tongs or pliers to hold the slide in case it either gets too hot or breaks. But, when
actually heating a slide during testing, I like to hold it in my fingers. If it starts getting
too hot I know it immediately! :~} Basically such tests require that you *warm* the
slide – not get it red-hot – in order to either promote evaporation of the liquid or
hasten a chemical reaction. And you do so *gently* – not *strongly.*
Heating solutions in a test tube is less of a hassle – they are designed to be heated,
even *strongly.* So you shouldn’t have to worry about them shattering when you put
the heat to them. But you do need to worry about following the instructions for a test –
not heating something strongly when the test calls for gentle heating. Again, you are
usually trying to either evaporate the liquid or hasten a reaction in it.
Gentle heating calls for pretty much the same approach as handling slides. Again, I
hold the tube in my hand, tipped at an angle, and don’t let it get too hot to hold –
keeping my fingers below the rim so they aren’t in the path of any fumes issuing from
the mouth of the tube.
Heating strongly requires a different approach. Here you want to put the heat to the
tube – but without actually bringing the contents to a boil. If you experiment a little
you’ll find that there is a curious phenomena which occurs when you heat a test tube:
Just before the liquid comes to a boil the tube begins to vibrate. So what you do is
heat the tube until you feel the vibration, then remove it from the heat for a few
seconds. Then put it back over the heat until it vibrates again. And so on until you’ve
achieved your purpose. After a while you’ll probably find yourself sort of waving the
test tube over the flame, keeping it just shy of boiling by dipping it in and out of the
flame with a continuous motion. Perfect!
DO NOT BRING ACIDS OR ACID SOLUTIONS TO A BOIL! You may only be
working with a few drops of solution, the danger relatively low, but – believe me –
you do not want to risk boiling off an acid all at once and getting a whiff of the fumes.
Or getting them in your eyes! (While there is still some risk in slowly evaporating
acid solutions, the fumes produced are much more dispersed and “diluted” with air.)
A few tests require heating the tube containing the test solution in a boiling water
bath. This means heating a beaker of water to a boil and suspending the test tube in it
for whatever time is required. A neat trick is to bend a medium or large sized paper
clip so one part forms a test tube holder and the other part forms a “hanger” that can
be hung on the edge of a beaker. Then you don’t need to hold the tube in the water by
hand in a test tube holder.
SILICATE FUSIONS
As noted above, most silicate minerals will not dissolve in the acids you can use
safely in a home lab. Some amateur mineral chemists avoid trying to test silicates for
this reason. But there is a method for freeing up the metallic ions in silicates that can
be done in the home lab. It is a bit tricky – and it won’t work for all silicates - but with
a little practice most people should be able to become proficient at it and thus expand
the list of minerals they can test. All it takes is sodium carbonate (Na2CO3), charcoal
blocks, and a propane torch or blowtorch. It’s a bit messy, but you can use charcoal
briquettes in place of charcoal blocks – you just have to scrape a flat on one side to
provide a stable base, and then gouge a small hollow in the opposite side. Make sure
the hollow is large enough to hold all the powder mixture you want to fuse. (It’s better
to fuse several small batches than to try for one large one.)
Mix a pinch of powdered silicate mineral with about four or five times that amount of
sodium carbonate powder. Place the powder mixture in the hollow on the charcoal
block (or briquette). Then heat the mixture with the blue flame of the torch until it
fuses into a solid globule on the charcoal. Once the globule cools, crush it back into a
powder. This powder should be dissolvable in hydrochloric acid – and the resulting
solution useable in a variety of tests for metallic ions. (If you find the powder does not
dissolve, try another fusion – perhaps using a smaller amount. Sometimes it takes a
couple tries to get a good fusion. If after several tries you can’t get a powder that
dissolves, you’ve probably come upon one of the silicates that’s difficult to fuse or
won’t fuse at all. That can be useful info in itself.)
QUANTITIES & MEASUREMENTS
I tend to think – and talk – in terms of “pinches” of powders and “drops” of liquids.
But what’s a “pinch”? A “drop”? I have a tiny lab spoon that holds about ¼ of the
volume of a Bayer aspirin. Maybe something like 5 to 7 milligrams. I call that a
“pinch.” A “tiny pinch” is what I can pick up with a pair of small tweezers and tap off
into the slide depression or test tube – maybe half a “pinch” or less. A “drop” is what
drips out of the end of a lab eyedropper when you squeeze the bulb just enough to
form a bead of liquid at the end that is big enough to drop off under its own weight.
Don’t ask me what that is in milliliters… (The micro-eyedropper is used for
producing tiny drops when you only have tiny amounts of mystery mineral powder to
work with, or when you need to slowly add solutions to achieve a desired degree of
acidity or alkalinity.)
Just thought we ought to define these – ahem! – highly technical and precise terms
before moving on. :~}
Also, this points out the fact that most qualitative testing for minerals is not really all
that persnickety when it comes to measurements. You don’t usually need precisely
controlled amounts of powders and liquids to get useable results. (Though some tests
do require measured amounts.) In quantitative tests measurements become more of an
issue. But we’re only talking rough quantities here – when we talk about them at all.
So you don’t have to get all in a lather about making sure you use exactly the right
amount of this to make that work.
SAFETY NOTE
Please read the previous posts on this topic before reading the information on tests
below. There is important information in those posts that you need to know before
you try doing any tests. If you try to short-cut things and dive into testing you could
get hurt – or hurt someone else.
Also please note that each post is being posted in reverse order: The lowest one was
posted first, and so on upwards to the last one. Read them in order; and if you print
them out for future reference number them in the proper sequence.
………………………………….THINK SAFE – BE
SAFE………………………………..
1) Start out with simple observations and tests. Though they are simple, they can be
telling:
...- Is it a metallic or submetallic mineral? Or is it nonmetallic?
...- If it is metallic or submetallic, will it readily mark a piece of paper? If it does, that
leads you to one group of minerals. And these can be sorted out based on the color of
their streak, hardness, and color of the mineral.
...-If it doesn’t mark paper, can you scratch it with a pocket knife? If it can, this leads
you to another group of minerals that can be sorted out the same way as the softer
group. If not, it leads you to a third group, also sortable the same way.
...The odds are in your favor that any metallic mineral at hand will fall into one of
those three groups, and that once you are looking at species of the right group you will
find the identity of your specimen in it.
...-If the mineral is non-metallic, does it have a definite colored streak? If it does, it
will lead you to a group of minerals that can be sorted based on the color of the streak,
the hardness, the color of the mineral, and other characteristics.
...-If the mineral does not have a colored streak, can you scratch it with your
fingernail? If you can, you end up at another group of minerals that can be further
subdivided based on whether or not the mineral has a prominent cleavage: If it does,
you are lead to a group of minerals that can then be sorted based on the number of
cleavages present, hardness, and color. If it doesn’t have a good cleavage you are lead
to yet another group of minerals that are again sortable based on their characteristics.
And so on... (The methodology eventual takes you all the way up to very hard non-
metallic minerals, including diamond. But I’m not going to lay it all out here – it is
available to you - now - elsewhere here at Bob's.)
3) If simple observations and tests, along with information provided by the matrix and
associated minerals, don’t get you an identification, get a bit more “aggressive” in
your search. Try things like specific gravity, crystal system and habit – maybe a few
of the easiest chemical tests, perhaps some of the easier optical observations.
...- Specific gravity is a powerful tool in mineral identification. One which all too few
collectors employ… Anyone who is at all serious about trying to identify minerals
needs to get the equipment and learn this technique. Period!
...- Understanding at least the basics of crystallography – the differences between
crystals in the seven crystal systems – is also a very powerful tool. With this under
your belt you should be able to identify many of the crystal shapes you encounter –
figure out at least which crystal system the mineral crystallizes in. Which effectively
eliminates any mineral which crystallizes in any of the six other systems…
...- Basic optical techniques are also powerful tools. Along with physical
characteristics, the optical properties of a mineral can narrow down the search for an
identity by a wide margin – in your favor. (Optical observations are my short coming
in mineralogy. I now wish I’d paid closer attention and tried harder when the prof was
trying to drill them into us...)
...- Flame and Bead tests are two more powerful tools. As Al O. has shown, they aren't
that hard to do. A little practice and you're off and running. I've used them for years, a
routine part of my mineral identification efforts. You should, too.
4) At some point you will undoubtedly run into something that defies identification
using the above tools. At that point you have to decide how much you want to get into
the nitty-gritty of mineral identification – go on to learn chemical testing, and
advanced optical observations, or find a lab to do it for you. I don’t think any of us
doing this seminar would say that chemical testing, or advanced optical work is for
everyone. They aren’t. But I happen to think that anyone who really sets their mind to
it can dope these out – become at least proficient enough to make good use of them.
But you have to want to, and you have to be patient – take things a slow step at a time.
If you do add these to your bag of tricks, there will be very few minerals you won’t be
able to identify – some of the real “toughies,” like telling the various amphiboles
apart, or the various zeolites, etc… Even some of the pros have a hard time with those
– resorting to even more advanced techniques, such as SEM analysis and X-ray
diffraction.
...- If you do decide to get into chemical testing, I strongly recommend that you take
the “least is best” approach outlined in that topic below. And work at being as
methodical in your testing using chemicals as you are (hopefully!) in your use of
simpler observations and tests. This is the safest, most economical, and surest way to
do chemical testing. The most practical by far... “Think Safe! – Be Safe!”